Process for the manufacture of resinous products capable of replacing natural resins.



I LJGROGNOT: 1 PROCESS FOR THE MANUFACTURE OF BESINOUS PRODUCTS CAPABLE OFREPLAOING NATURAL RESINS.

AL'PLIOATIDH IIBED SEPT. 5, 1907,

A 7 o kin m LEON GROGNOT, F

ame srA-TEs PATENT oFFIcE;

success FOR THE mmurac rnnn' or ansrnotisrrionucrs camara- 0F Rnrmeme PARIS, FRANCE, ASSI-GNOR 'ro soont'ria DITE: LES rnonurrs onmi uEs DEOROISSY LIMITED, 0 PARIS, FRANCE, A FIRM.

NATURAL meme.

Specification of Letters Patent.

Patented Dec. 8, 1903;

Application. filed se amter 5, 1-901. seam no. 391,638.

To all whom "it may concern:

" Be'it known that I, Llion GROGNOT, a citizen of the French Republic, residing at 18 Rue Labat,'Paris, France, chemist, have invented certain new and useful Improvements in and-Relating to Processes for the Mann-L facture of Resinous Products Capable of Replacing Natural Resins, of which the following is a specification. e I

This invention has for its object a process for the manufacture of resinous products capable of replacing natural resins, such as gum-lac, succin, copal or others. I lt is known that the phenols have the property of, combining with the aldehydes under the'influence of catalytic agents (such as mineral or organic acids, alkalme or other bases) for formmg various resins analogous to the natural: resins in their properties. Nevertheless the action of these" catalytic agents is diflicult to control and goes be- .yond what is required. .The present process of which the under the influence of heat, and o permits of obviating this defect.

The accompanying drawing, which is given by way of example, illustrates a constructional form of an apparatus by means process may be carried into practice for o taining a resinous product analogous to gum-lac.

The process forming the object of this-invention consists broadly in first of all combining the aldehyde with anintermediate agent or determinant such as a glycerin,

a catalytic agent such ashydrochloric acid; then in adding a phenol which regenerates the glycerin by a second reaction presenting no violence, and gives a thick oil which is treated by' washings, dehydration and moderate heating, the resinous product being finally obtained. y 7

In order to obtain a product analogous to gum-lac for example, the following is'the preferred method z -In an enameled cast iron vessel a there are mixed: 200 kgs.. of

glycerin with 200 kgs. of formic aldehyde, 1

then 30 to 40 kgs. of hydrochloric acid at 21 or 22 Baum. The whole is heated by means .ofan appropriate source of heat until islight 'ebullition' occurs; this continues of itself withoutfire, owing to the c0mbina.- tionof the glycerin with the aldehyde. At

"the end of the reaction the heat is again It is desirable to rovide the vessel with a cover 6 and to direct the vapors into a cooled ascending coil 0 in order to prevent the loss of an substance which ma be carried along. (loolin'g to about 80 is then allowed to take place and about 200 kgs. of white phenic acid of a high standard is then added to the mass. After mixing and without heatin a reaction is produced with slight ebul ltion which continues for a certain period. After this" a thick oil is formed above a lycerinousliquid. This latter is separate the oil is washed several times in neighborhood 0 100 0., either in the at-- mosphere'or in 'vacuo. Finally, the oil is heated to approximately 150 and maintained about this tem erature untila test quantity withdrawn in icates that the cooled resin is hard and brilliant. The resin may then be cast into thin sheets, beads or sticks,- as desired.

The process presents the advantage of rendering the o eration uniform and of avoiding any vio ent reaction which might give rise to useless accessory products or products whichwould be harmful ,to the products that it is sought to obtain. The glycerin contained in the washing waters may be evaporated and regenerated so as to serve again.

In place of formic aldehyde any other aldehyde or substance fulfilling the same functlon may be employed; similarly the glycerin and the phenol may be replaced by bodies-of-any kind of the corresponding series or fulfilling the same functions. It is before casting it, suitable proportions of vegetable'or animal wax and gluten to impart to the gum-lac or other resm all the properties of ordinary lac. I

:The process serves for the manufacture of resinous products suited for replacing resins of all kinds.

Having now particularly. described and ascertainecLthe nature of my said invention and in what manner the same is to be'perous products by the action of phenols on aldehydes, consisting in first combining the aldehyde with an intermediary substance, the reaction being facilitated by the addition ofva catalytic agent which merely acts' by its presence, and then causing the phenol to decompose the combination of the aldehyde and the intermediary substance and to regenerate-the latter.

2. A process for the manufacture of resinous products consisting'in combining an aldehyde with intermediary substances under the influence of heat and of a catalytic agent, regenerating the intermediary substances by the action of a phenol and pro- -oily compound by washing and heating.

4. A method of obtaining a resin analogous to gum-lac consisting in combining ormic aldehyde with glycerin, the reaction being facilitated by the presence of hydrochloric acid, and then causing phenic acid to act on the combination of formic aldehyde and glycerin, thus regenerating the glycerin day of August 1907.

and combining with the aldehyde in the shape, of a thick oil.

5. A method of obtaining a product analogous to gum-lac, consisting in combining formic aldehyde with glycerin in the presence of a small quantity of hydrochloric acid at 21 or 22 Baum, in heating to the point of slight ebullition, adding phenic acid after the mass has'been allowed to cool to about 80 (1., then separating the thick oil formed from the regenerating glycerin, and condensing said oil to a hard matter by heatin 6. A method of obtaining a product ana ogous to gum-lac consisting in combining equal proportions of formic aldehyde and glycerin in the presence of a small quantity 7 of hydrochloric acid, heatin to the point of slight ebullition, allowing file mass to cool to about 80 (1., then adding at once phenic acid e ual in proportion to the foregoing two so stances, separating from the regenerated glycerin the thick oil formed, w llCh is dehydrated by heating to about 100 (3., and which is condensed to a hard consistency in heating it to about 150 C. I

In testimony whereof I have hereunto placed my hand at Paris, France, this 21st LEON eRooNoT.

- In thepresence of two witnesses CH. DE LAVIGEI, HENRY SOHWAB. 

